A production system of isochlorogenic acid B

Abstract

The utility model discloses a production system of isochlorogenic acid B, including dissolving jar, reaction jar, first buffer tank, first concentration jar, primary extraction jar, secondary extraction jar, macroporous adsorption resin column, second buffer tank, first drying jar, primary crystallization jar, first plate and frame filter, secondary crystallization jar, second plate and frame filter, second drying jar and product storage tank, the dissolving jar is connected with first purified water storage tank and first pH regulator storage tank, the first buffer tank is connected with second pH regulator storage tank, the secondary extraction jar is connected with third pH regulator storage tank, the macroporous adsorption resin column is connected with second purified water storage tank, ethanol storage tank, the second buffer tank is connected with fourth pH regulator storage tank, the production system takes sweetleaf chrysanthemum polyphenol product as raw material, separates and purifies through isomerization reaction, multistage extraction, resin adsorption, multistage crystallization, obtains high purity isochlorogenic acid B, and the waste liquid in the process is fully recycled, and is economic and environmental protection.

Description

Technical Field

[0001] This utility model relates to the field of isochlorogenic acid B preparation technology, specifically to a production system for isochlorogenic acid B. Background Technology

[0002] Isochlorogenic acid B, as an important natural phenolic acid compound, has significant antioxidant, anti-inflammatory and antibacterial biological activities, and has broad application prospects in the fields of medicine, food and cosmetics.

[0003] Currently, the preparation of isochlorogenic acid B mainly relies on extraction from plants. Conventional extraction processes typically involve reflux extraction with alcohol solvents, resin enrichment, and purification by chromatography. However, these methods have the following limitations: First, the reliance on column chromatography for monomer purification is cumbersome, time-consuming, and requires large amounts of organic solvents, resulting in high costs and making it difficult to meet the needs of large-scale industrial production. Second, the chlorogenic acid compounds in the extract have similar physicochemical properties, making separation difficult and leading to low yields and purity of isochlorogenic acid B, thus affecting its applications. Utility Model Content

[0004] The technical problem to be solved by this utility model is to provide a production system for isochlorogenic acid B, which addresses the shortcomings of the existing technology. The system uses stevia polyphenols as raw materials and separates and purifies them through isomerization reaction, multi-stage extraction, resin adsorption and multi-stage crystallization to obtain high-purity isochlorogenic acid B. The waste liquid in the process is fully recycled and reused, which is economical and environmentally friendly.

[0005] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0006] A production system for isochlorogenic acid B includes a dissolving tank, a reaction tank, a first buffer tank, a first concentration tank, a primary extraction tank, a secondary extraction tank, a macroporous adsorption resin column, a second buffer tank, a first drying tank, a primary crystallization tank, a first plate and frame filter, a secondary crystallization tank, a second plate and frame filter, a second drying tank, and a product storage tank, all connected by pipelines.

[0007] The dissolving tank is connected to a first purified water storage tank and a first pH adjuster storage tank; the first buffer tank is connected to a second pH adjuster storage tank; the first-stage extraction tank and the second-stage extraction tank are both connected to water-saturated ethyl acetate storage tanks; the second-stage extraction tank is also connected to a third pH adjuster storage tank; the macroporous adsorption resin column is connected to a second purified water storage tank and an ethanol storage tank; the second buffer tank is connected to a fourth pH adjuster storage tank; the first-stage crystallization tank is connected to an acetone storage tank; and the second-stage crystallization tank is connected to a third purified water storage tank.

[0008] Preferably, the extraction phase outlet of the primary extraction tank is connected to a waste liquid recovery tank.

[0009] Preferably, the extract phase outlet of the secondary extraction tank is connected to the dissolving tank via a second concentration tank.

[0010] Preferably, the filtrate outlet of the first plate and frame filter is connected to the first buffer tank via a third concentration tank.

[0011] Preferably, the filtrate outlet of the second plate and frame filter is connected to the second buffer tank.

[0012] Preferably, the reaction vessel is provided with a first stirring device, the first stirring device including a first stirring shaft provided in the reaction vessel, the first stirring shaft being connected to a first stirring motor provided at the top of the reaction vessel, and the first stirring shaft being provided with a plurality of downwardly inclined first stirring blades.

[0013] Preferably, the primary crystallizer is provided with a second stirring device, the second stirring device including a second stirring shaft provided in the primary crystallizer, the second stirring shaft being connected to a second stirring motor provided at the top of the primary crystallizer, the second stirring shaft being provided with a plurality of second stirring blades, and the second stirring blades being connected to scrapers that abut against the inner wall of the primary crystallizer via flexible rods.

[0014] By adopting the above technical solution, this utility model has at least the following beneficial effects:

[0015] This invention provides a production system for high-purity isochlorogenic acid B. The system prepares high-purity isochlorogenic acid B from stevia polyphenol products through processes such as dissolution, isomerization reaction, multi-stage extraction, macroporous adsorption resin treatment, and multi-stage crystallization. It is suitable for large-scale production.

[0016] In this production system, the extraction phase outlet of the primary extraction tank is connected to a waste liquid recovery tank, and the extraction phase outlet of the secondary extraction tank is connected to a dissolving tank through a second concentration tank. This allows unreacted materials or intermediate products to be recovered and reused, reducing raw material consumption and increasing product yield.

[0017] In this production system, the filtrate outlet of the first plate and frame filter is connected to the first buffer tank through the third concentration tank, and the filtrate outlet of the second plate and frame filter is connected to the second buffer tank. This allows the effective components in the crystallization mother liquor to be recovered, reducing waste liquid discharge and making it economical and environmentally friendly.

[0018] This production system uses a primary extraction tank and a secondary extraction tank, combined with a macroporous adsorption resin column, to effectively remove impurities and selectively adsorb isochlorogenic acid B, thereby improving product purity.

[0019] In this production system, the primary and secondary crystallizers perform multi-stage crystallization on the crude product. By optimizing the crystallization conditions, the crystals are further purified, and the product purity is improved.

[0020] This production system is equipped with multiple pH adjuster storage tanks to effectively regulate the pH of the solution at each stage, optimize reaction conditions and crystallization environment, reduce side reactions, and improve product quality and purity.

[0021] The first stirring device in this production system can promote thorough mixing of materials, prevent sedimentation, and improve reaction efficiency; the second stirring device can not only improve crystallization efficiency, but also prevent crystals from adhering to the inner wall, ensure uniform heat transfer, make the crystallization process more controllable, and thus reduce product loss. Attached Figure Description

[0022] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0023] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of this utility model;

[0024] Figure 2 yes Figure 1 Enlarged structural diagram at point A;

[0025] In the diagram, 1. Dissolving tank; 2. Reaction tank; 3. First buffer tank; 4. First concentration tank; 5. First extraction tank; 6. Second extraction tank; 7. Macroporous adsorption resin column; 8. Second buffer tank; 9. First drying tank; 10. First crystallization tank; 11. First plate and frame filter press; 12. Second crystallization tank; 13. Second plate and frame filter press; 14. Second drying tank; 15. Product storage tank; 16. First purified water storage tank; 17. First pH adjuster storage tank; 18. Second pH adjuster storage tank; 19. Water. 20. Saturated ethyl acetate storage tank; 21. Third pH adjuster storage tank; 22. Second purified water storage tank; 23. Ethanol storage tank; 24. Fourth pH adjuster storage tank; 25. Acetone storage tank; 26. Third purified water storage tank; 27. Second concentration tank; 28. Third concentration tank; 29. ​​First stirring shaft; 30. First stirring motor; 31. First stirring blade; 32. Second stirring shaft; 33. Second stirring motor; 34. Second stirring blade; 35. Flexible rod; 36. Scraper; 37. Waste liquid recovery tank. Detailed Implementation

[0026] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0027] Example 1

[0028] like Figure 1 and 2 As shown, a production system for isochlorogenic acid B includes a dissolving tank 1, a reaction tank 2, a first buffer tank 3, a first concentration tank 4, a primary extraction tank 5, a secondary extraction tank 6, a macroporous adsorption resin column 7, a second buffer tank 8, a first drying tank 9, a primary crystallization tank 10, a first plate and frame filter 11, a secondary crystallization tank 12, a second plate and frame filter 13, a second drying tank 14, and a product storage tank 15, all connected by pipelines.

[0029] The dissolving tank 1 is connected to a first purified water storage tank 16 and a first pH adjuster storage tank 17; the first buffer tank 3 is connected to a second pH adjuster storage tank 18; the first-stage extraction tank 5 and the second-stage extraction tank 6 are both connected to a water-saturated ethyl acetate storage tank 19; the second-stage extraction tank 6 is also connected to a third pH adjuster storage tank 20; the macroporous adsorption resin column 7 is connected to a second purified water storage tank 21 and an ethanol storage tank 22; the second buffer tank 8 is connected to a fourth pH adjuster storage tank 23; the first-stage crystallization tank 10 is connected to an acetone storage tank 24; and the second-stage crystallization tank 12 is connected to a third purified water storage tank 25.

[0030] The above-mentioned production system recovers high-purity isochlorogenic acid B from stevia polyphenol products through dissolution, isomerization reaction, primary extraction, secondary extraction, resin adsorption, primary crystallization, and secondary crystallization.

[0031] In this embodiment, the extract phase outlet of the primary extraction tank 5 is connected to a waste liquid recovery tank 36; the extract phase outlet of the secondary extraction tank 6 is connected to the dissolving tank 1 via a second concentration tank 26. The extract phases from the primary and secondary extraction processes are concentrated in the second concentration tank 26, and the concentrated material is returned to the dissolving tank 1 for further processing, thereby improving resource utilization and reducing production costs.

[0032] In this embodiment, the filtrate outlet of the first plate and frame filter 11 is connected to the first buffer tank 3 via the third concentration tank 27; the filtrate outlet of the second plate and frame filter 13 is connected to the second buffer tank 8. This configuration effectively recovers residual isochlorogenic acid B from the crystallization mother liquor, contributing to an improved overall yield of isochlorogenic acid B.

[0033] In this embodiment, the reaction vessel 2 is equipped with a first stirring device, which includes a first stirring shaft 28 disposed within the reaction vessel 2. The first stirring shaft 28 is connected to a first stirring motor 29 disposed at the top of the reaction vessel 2. The first stirring shaft 28 is provided with a plurality of downwardly inclined first stirring blades 30. This arrangement can improve heat exchange efficiency, thereby increasing reaction efficiency.

[0034] In this embodiment, a second stirring device is provided inside the primary crystallization tank 10. The second stirring device includes a second stirring shaft 31 disposed inside the primary crystallization tank 10. The second stirring shaft 31 is connected to a second stirring motor 32 disposed at the top of the primary crystallization tank 10. The second stirring shaft 31 is provided with a plurality of second stirring blades 33. The second stirring blades 33 are connected to scrapers 35 that abut against the inner wall of the primary crystallization tank 10 through flexible rods 34. The above arrangement can scrape the tank wall in real time while stirring, effectively preventing scale formation on the tank wall and ensuring stable heat transfer efficiency and crystallization process.

[0035] The process of producing isochlorogenic acid B using this production system is as follows:

[0036] S1: Add the stevia polyphenol product to dissolving tank 1, add purified water and stir until the solid dissolves, adjust the pH of the solution to obtain the first solution to be treated;

[0037] S2: The liquid to be treated enters the reaction tank 2, is heated and stirred to react. After the reaction is completed, the reaction liquid enters the first buffer tank 3, the pH is adjusted, and then it enters the first concentration tank 4 for concentration. After that, it enters the first extraction tank 5, where water-saturated ethyl acetate is added for extraction. The extract phase is recovered to the waste liquid recovery tank 36 for the preparation of low-content polyphenols. The raffinate phase enters the second extraction tank 6, the pH is adjusted, and water-saturated ethyl acetate is added for second-stage extraction. The extract phase is desolventized in the second concentration tank 26 and then recycled to the dissolving tank 1.

[0038] S3: The raffinate from the secondary extraction is adsorbed onto a macroporous adsorption resin column 7, then treated with purified water as top feed, and finally eluented with a certain concentration of ethanol solution. The eluent enters the second buffer tank 8 to adjust the pH, and then enters the first drying tank 9 for drying. The dried material enters the first crystallization tank 10, where acetone is added and stirred until the solid dissolves. Then, it is stirred and crystallized at room temperature. The first crystallization liquid is filtered through the first plate and frame filter press 11. The filtrate is desolventized in the third concentration tank 27 and then circulated back to the first buffer tank 3. The filter cake enters the second crystallization tank 12, where purified water is added and heated and stirred until the solid dissolves. Then, it is cooled and crystallized. The second crystallization liquid is filtered through the second plate and frame filter press 13. The filtrate is circulated back to the second buffer tank 8. The filter cake is dried in the second drying tank 14 and then stored in the product storage tank 15.

[0039] The above description of the disclosed embodiments enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A production system for isochlorogenic acid B, characterized in that: It includes a dissolving tank, a reaction tank, a first buffer tank, a first concentration tank, a first-stage extraction tank, a second-stage extraction tank, a macroporous adsorption resin column, a second buffer tank, a first drying tank, a first-stage crystallization tank, a first plate and frame filter, a second-stage crystallization tank, a second plate and frame filter, a second drying tank, and a product storage tank, all connected by pipelines. The dissolving tank is connected to a first purified water storage tank and a first pH adjuster storage tank; the first buffer tank is connected to a second pH adjuster storage tank; the first-stage extraction tank and the second-stage extraction tank are both connected to water-saturated ethyl acetate storage tanks; the second-stage extraction tank is also connected to a third pH adjuster storage tank; the macroporous adsorption resin column is connected to a second purified water storage tank and an ethanol storage tank; the second buffer tank is connected to a fourth pH adjuster storage tank; the first-stage crystallization tank is connected to an acetone storage tank; and the second-stage crystallization tank is connected to a third purified water storage tank.

2. The isochlorogenic acid B production system according to claim 1, characterized in that: The extraction phase outlet of the primary extraction tank is connected to a waste liquid recovery tank.

3. The isochlorogenic acid B production system according to claim 1, characterized in that: The extract phase outlet of the secondary extraction tank is connected to the dissolving tank via a second concentration tank.

4. The isochlorogenic acid B production system according to claim 1, characterized in that: The filtrate outlet of the first plate and frame filter is connected to the first buffer tank through the third concentration tank.

5. The isochlorogenic acid B production system according to claim 1, characterized in that: The filtrate outlet of the second plate and frame filter is connected to the second buffer tank.

6. The isochlorogenic acid B production system according to claim 1, characterized in that: The reaction vessel is equipped with a first stirring device, which includes a first stirring shaft located inside the reaction vessel. The first stirring shaft is connected to a first stirring motor located at the top of the reaction vessel. The first stirring shaft is provided with a plurality of downwardly inclined first stirring blades.

7. The isochlorogenic acid B production system according to claim 1, characterized in that: The primary crystallization tank is equipped with a second stirring device, which includes a second stirring shaft located inside the primary crystallization tank. The second stirring shaft is connected to a second stirring motor located at the top of the primary crystallization tank. The second stirring shaft is equipped with a plurality of second stirring blades, and the second stirring blades are connected to scrapers that abut against the inner wall of the primary crystallization tank via flexible rods.

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